The method of obtaining complex diesters of terephthalic acid and diols polyesters

 

(57) Abstract:

The invention relates to methods for complex diesters of terephthalic acid and diodes of polyesters. The method consists in the depolymerization of a complex of the polyester in the presence of an interesterification catalysts for the above-mentioned complex of the polyester and in the presence of ester and subsequent transesterification of the reaction mixture with obtaining complex diapir terephthalic acid by reaction with a monohydroxy alcohol. Using the new method, you can get the original monomers for obtaining polyesters rapidly and under mild reaction conditions. 11 C.p. f-crystals.

The invention relates to a new method of obtaining complex diesters of terephthalic acid and diodes from waste polyesters. Along with polyethylene terephthalate (hereinafter PET) in trade there are other polyesters. The term "complex polyester" means a polyester acid component which contains at least part of the monomers terephthalic acid. From the total number of PET in about 16 million tons per year produced at the present time, only a very small number of Podwale the AET total processing capacity. Reapply complex polyester after its use as a polymer represented only a relatively possible, this means that you can only use relatively small quantities for the purposes of lower quality applications, "WM on". Therefore, there is a need for suitable methods to decompose the polymer by chemical means so that the derived monomers, after cleaning, you might use the equivalent conventional source materials "IR-WM"

In principle, a complex polyester can be converted into terephthalic acid or in complex fluids terephthalic acid, as for example, in the terephthalate (hereinafter DMTF). Terephthalic acid can be cleared only by recrystallization and / or adsorption, and filtration of the entire solution in large quantities is from a technological point of view is very (very) expensive. Therefore, it is difficult soluble contaminants to separate from the terephthalic acid is not in the required scope, which limits the use of the obtained terephthalic acid. DMTF can be as recrystallization and distillation. Therefore, it is possible to ensure the purity required for Prica for reuse complex polyester through DMTF due to more favorable conditions cleaning has the advantage before processing through terephthalic acid, it needed a cost-effective way that would work continuously and which could transform large amounts of complex polyester with possible mild conditions.

It is known that a complex of the polyester can be decomposed with methanol at temperatures from 100 to 300oC and pressures up to 150 ATM to DMTF (application for U.S. patent 3.776.945). The disadvantage of this method is that you have to live with for a very long time along with high blood pressure. This disadvantage can be mitigated by applying steam (application for U.S. patent N 3321510), and using the interesterification catalysts (application for U.S. patent 03037050) IN DE-A-1,003,714 has been described that the decomposition of the polyester to DMTF considerably accelerated by using methanol and catalysts interesterification in the presence of DMTF. Similarly with this application for U.S. patent 5051528 describes the transformation of PET in DMTF in the presence of catalysts in the transesterification with methanol is accelerated by the fact that PET is additionally added to the oligomers and at the same time spend processing at supercritical conditions paraetamol. The reaction is carried out in such a way that distilled DMTF, glycol and excess methanol. Therefore, non-volatile ingredients in PET going into the reactor is

So previously known methods of utilization of the components of the acid and alcohol from polyesters differ in the use of expensive measures. So on the application for U.S. patent 5.051.528 need to make solid PET in the reactor, treated with supercritical steam methanol and under pressure, if I want to get the reaction continuously. According to DE-A-1,003,714 continuous method of carrying out the reaction is possible.

Common to both methods is that the decomposition of polyethylene terephthalate with methanol in the presence of DMTF or oligomers. Based on these previously known methods, the present invention was to develop a method that would allow the transformation of large quantities of complex polyester, quickly, with possible mild conditions in complex fluids terephthalic acid and diols, mainly in DSTF and ethylene glycol, avoiding the above-described technological difficulties, and this method is most advantageously carried out as continuous. Unexpectedly found that polyesters can be subjected to depolymerization with esters of monohydroxy alcohols in the presence of catalysts interesterification, and depolymerization occurs the advantage is on the aromatic dimethylterephthalate (hereinafter DMADV). If DMTF use in insufficient quantity in relation to PET, get oligomers with groups challenging methyl ester as a terminal group. Oligomers and DMADV subjected to interesterification in equilibrium with methanol to DMTF. Found that the stage of depolymerization in the presence of an interesterification catalyst is much faster. If carried out the reaction between the polymer and the complex ester in the presence of catalysts in the transesterification reaction can be carried out without high pressure, and depending on the set temperature of the reaction, to end in a few minutes. By dividing both reactions, decomposition of the polymer and interesterification, you can develop a continuous way with simple technology.

Therefore, the invention relates to two-stage method for producing a Monomeric complex diesters of terephthalic acid and diols by depolymerization of a complex of the polyester with esters of monohydroxy alcohols in the presence of catalysts for the transesterification and subsequent transesterification of depolymerised with a monohydroxy alcohol. For carrying out the method according to the invention, PET-granulate make in the presence of catalysts pretermitted. While the interesterification catalysts can be formed from PET-granulate and/or they can be added. The granulate is separated by splitting up and get melt with the ability to be transported by the pump. It is introduced in preterition reactor, which process from the bottom using a pair of methanol. The excess methanol and the resulting glycol is brought out through the upper part of the reactor, while DMTF and contamination of PET is distilled through a sump. The product obtained in the sump, is distilled under further purification. The head fraction is distilled off by distillation.

A significant advantage of this method is that water is allocated in the process of depolymerization, mostly evaporated. The partial hydrolysis with the release of methanol. The resulting acid is again subjected to the esterification stage interesterification with formation water. When the single-stage process on the application for U.S. patent 5051528 the contrary, all imported PET-granulate water is absorbed by the mixture of methanol, glycol and it should distillation to select.

As the source material used all polyesters containing terephthalic acid.It is,therefore, preferred examples include polybutylene terephthalate and especially polyethylene terephthalate. Examples of spoliation are sopoliarilenefirketony, which, together with terephthalic acid and ethylene glycol include aliphatic dicarboxylic acids such as adipic acid or sabotinova acid as the acid component, and/or aliphatic diols such as di-ethylene glycol or butyleneglycol as a component of alcohol. As of ester phase depolymerization mainly use complex alkilany ether, mainly complex diakidoy ester of an aromatic dicarboxylic acid.

Examples of complex alilovic esters are complex alkalemia esters of aliphatic, cycloaliphatic, alifaticheskih or especially aromatic monocarboxylic or Scarborough acids. Preferred esters with altergroup with 1-6 carbon atoms, especially complex ethyl esters, and most preferred methyl esters.

As the acid component for complex alilovic esters are suitable, for example, formic acid, acetic acid, propionic acid, butyric acid, adipic acid, sabotinova acid or cyclohexanecarbonyl acid. Especially as the acid component for complex alilovic is but terephthalic acid. Examples of preferred esters are dimethyltotal, particular preference is given to the exporter. Ester is used in General in amounts of from 0.5 to 10 mmol, relative to one mole of the complex polyester. Mainly used from 1 to 5 mol.

You can also use a mixture of esters. As catalysts for the transesterification use all compounds suitable for this purpose, or a mixture of such compounds. Examples of preferred interesterification catalysts are manganese acetate, zinc oxide, zinc acetate, zinc chloride or magnesium oxide or a mixture of such compounds, as well as other acidic catalysts interesterification.

The catalysts used are useful in amounts of from 10 to 500 ppm, relative to the complex of the polyester. Found that the depolymerization is carried out in a noticeable extent at a temperature ranging from the melting point of the complex ester. In the case of DMTF choose the temperature of the depolymerization at least 140oC. the reaction Rate increases with reaction temperature. The solubility of water in DMTF decreases with reaction temperature. In the case of DMTF chosen as the area of t is eakly finish also during her without increased pressure for several minutes. Allocated water is mostly evaporated.

The depolymerization can be carried out in solution or mainly in the melt, it can mostly be without high pressure or at a pressure of, for example, at a pressure of from 1 to 30 bar, mostly from 1 to 5 bar.

As the solvent used, for example, DMSO, DMF, N-methyl-pyrrolidone, triamide, hexamethylphosphoric acid or other solvent in which the complex polyester is at least partially soluble.

For further course of the reaction can be observed by controlling the melt viscosity or the viscosity of the solution in the reaction mixture. Equilibrium in the melt is usually achieved as soon as the viscosity of the melt approaches the value of the viscosity of ester used, the choice of stoichiometry, so that the PET can be completely split, that is, when the stoichiometry ratio DMTF:PET 1:1. Needless to say that the splitting can be maintained in the first stage, especially in a continuous process, and also at higher viscosities.

For interesterification can, in principle, in the method according to the invention, to use almost all monatomic sleep is such, aromatic or especially aliphatic alcohols.

Examples of such alcohols include cyclohexanol, metilaritromicin, phenol, methanol, ethanol, propanol, butanol, pentanol and hexanol. At the stage of interesterification mostly use alkilany alcohol with 1 to 6 carbon atoms, mainly methanol.

Monohydroxy alcohol is used in General in amounts of from 2 to 20 mol, relative to one mole of the complex polyester. Mainly used from 5 to 10 mol. Monohydroxy alcohol after separation from the obtained diol mainly used on stage pereeterifikacii in a cyclic process.

Stage interesterification can be carried out at temperatures between 140 and 300oC and without high pressure or at elevated pressure, for example, at a pressure of between 1 to 20 bar. As a rule, mainly the two stage process is carried out continuously.

In the variant with the greatest advantages of the method according to the invention, the part of the received complex diapir terephthalic acid again enter the stage of depolymerization.

Example 1. In the flow reactor of continuous operation at the same time introducing streams of the following compounds: 3 mol liquid DMTF, 1 mol actionnow mixture in the reactor is 40 minutes

The resulting mixture of products from MADTV in DMF continuously served in preterition column, in which bottom-down pairs of methanol. From the upper part of the reactor is continuously distilled off the mixture of methanol / glycol, which is partially used as phlegmy, and partially shared through another column. Glycol is separated: methanol injected into preterition column. From the cube preterition columns continuously divert DMTF, part of which is served back to the reactor, and the other part serves in a distillation column.

Example 2. In the flow reactor served continuously flows the following compounds: 1.5 mol DMTF, 1 mol PETP-graduate and 400 ppm of solid manganese acetate. The reaction temperature is 180oC the pressure in the reaction time to 5 bar. The average residence time of the reaction mixture in the reactor is 30 minutes the resulting mixture of products continuously further processed according to example 1.

1. The method of obtaining complex diesters of terephthalic acid and diols by depolymerization of a complex of the polyester by heating in the presence of ester and subsequent transesterification when heated, wherein the depolymerization is carried out in the presence of a catalyst pogo alcohol and dicarboxylic acid, with subsequent supply of mixture in preterition column, the transesterification is carried out using a pair of monohydroxy alcohol with the formation of complex diapir terephthalic acid and diol.

2. The method according to p. 1, characterized in that as a complex polyester used terephthalate.

3. The method according to p. 1 or 2, characterized in that the quality of ester during the depolymerization use complex diakidoy ester of an aromatic dicarboxylic acid.

4. The method according to p. 3, characterized in that the complex ester is terephthalate.

5. The method according to p. 1, characterized in that as a catalyst for interesterification using manganese acetate, zinc oxide, zinc acetate, zinc chloride, or magnesium oxide or a mixture of such compounds.

6. The method according to p. 2, wherein the depolymerization is carried out at 140 250oWith no high pressure in the presence of an interesterification catalyst under item 5.

7. The method according to p. 1, characterized in that the control over the reaction is carried out by measuring the viscosity of the melt.

8. The method according to p. 1, characterized in that the monohydroxy alcohol on stage interesterification is alkilany alcohol is avodat at a temperature of 140 300oC and a pressure of 1 to 20 bar.

10. The method according to p. 1, characterized in that at the stage of interesterification excess monohydroxy alcohol is distilled together with diola formed of a tough polyester, and remaining in the sediment complex fluids terephthalic acid is then purified using distillation.

11. The method according to p. 1, characterized in that the phase depolymerization and stage interesterification is conducted continuously.

12. The method according to p. 1, characterized in that the part of the received complex diapir terephthalic acid again enter the stage of depolymerization.

 

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37 cl, 9 ex

FIELD: chemistry.

SUBSTANCE: invention relates to an improved method, by which the carboxylic acid/diol mixture, that is suitable as the initial substance for the manufacture of polyester, obtained from the decolourised solution of carboxylic acid without actually isolating the solid dry carboxylic acid. More specifically, the invention relates to the method of manufacturing a mixture of carboxylic acid/diol, where the said method includes the addition of diol to the decolourised solution of carboxylic acid, which includes carboxylic acid and water, in the zone of the reactor etherification, where diol is located at a temperature sufficient for evaporating part of the water in order to become the basic suspending liquid with the formation of the specified carboxylic acid/diol mixture; where the said carboxylic acid and diol enter into a reaction in the zone of etherification with the formation of a flow of a complex hydroxyalkyl ether. The invention also relates to the following variants of the method: the method of manufacture of the carboxylic acid/diol mixture, where the said method includes the following stages: (a) mixing of the powder of damp carboxylic acid with water in the zone for mixing with the formation of the solution of damp carboxylic acid; where the said carboxylic acid is selected from the group, which includes terephthalic acid, isophthatic acid, naphthalenedicarboxylic acid and their mixtures; (b) discolourisation of aforesaid solution of damp carboxylic acid in the zone for reaction obtaining the decolourised solution of carboxylic acid; (c) not necessarily, instantaneous evaporation of the said decolourised solution of carboxylic acid in the zone of instantaneous evaporation for the removal of part of the water from the decolourised solution of carboxylic acid; and (d) addition of diol to the decolourised solution of carboxylic acid in the zone of the reactor of the etherification, where the said diol is located at a temperature, sufficient for the evaporation of part of the water in order to become the basic suspending liquid with the formation of the carboxylic acid/diol mixture; where the aforesaid carboxylic acid and diol then enter the zone of etherification with the formation of the flow of complex hydroxyalkyl ether; and relates to the method of manufacture of carboxylic acid/diol, where the said method includes the following stages: (a) the mixing of the powder of damp carboxylic acid with water in the zone for mixing with the formation of the solution of carboxylic acid; (b) discolourisation of the said solution of damp carboxylic acid in the reactor core with the formation of the decolourised solution of carboxylic acid; (c) crystallisation of the said decolourised solution of carboxylic acid in the zone of crystallisation with the formation of an aqueous suspension; and (d) removal of part of the contaminated water in the aforesaid aqueous solution and addition of diol into the zone of the removal of liquid with the obtaining of the said carboxylic acid/diol mixture, where diol is located at a temperature sufficient for evaporating part of the contaminated water from the said aqueous suspension in order to become the basic suspending liquid.

EFFECT: obtaining mixture of carboxylic acid/diol.

29 cl, 4 dwg

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